CN105875607A - Pendimethalin micro-capsule suspending agent and preparation method thereof - Google Patents
Pendimethalin micro-capsule suspending agent and preparation method thereof Download PDFInfo
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- CN105875607A CN105875607A CN201610320446.1A CN201610320446A CN105875607A CN 105875607 A CN105875607 A CN 105875607A CN 201610320446 A CN201610320446 A CN 201610320446A CN 105875607 A CN105875607 A CN 105875607A
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- suspending agent
- pendimethalin
- microcapsule suspending
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
- A01N33/18—Nitro compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
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- Pest Control & Pesticides (AREA)
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- Engineering & Computer Science (AREA)
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- Agricultural Chemicals And Associated Chemicals (AREA)
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Abstract
The invention relates to a pendimethalin micro-capsule suspending agent and a preparation method thereof. The pendimethalin is taken as the micro-capsule core of the pendimethalin micro-capsule suspending agent and the content thereof is 10-450g/L; polyuria or polyurethane is taken as a micro-capsule wall of the pendimethalin micro-capsule suspending agent and the content thereof is 20-100g/L; the pendimethalin micro-capsule suspending agent also contains 20-100g/L emulsifier, 20-60g/L dispersing agent, 30-100g/L antifreezing agent, 1-10g/L viscosity modifier and 2-15g/L antifoaming agents and the balance of water. The pendimethalin micro-capsule suspending agent can solve the problem that the liquid preparation is easy to color and pollute the drug applying equipment; the agent does not contain the solvent and is environment-friendly; the compound of dispersing agent and emulsifier adopted by the invention can solve the problem of system creaming caused by coarse crystal easily generated by the low melting point compound following the temperature fluctuation; according to the preparation method provided by the invention, the temperature control is adopted, the operation is performed under normal pressure, no catalyst is used, the process is simple, no special equipment is required and the cost is low.
Description
Technical field
The present invention relates to field of pesticide preparation, be specifically related to a kind of Pendimethalin microcapsule suspending agent
And preparation method thereof.
Background technology
Pendimethalin (Pendimethalin), belongs to dinitroaniline herbicide, sterling
For orange crystals solid, fusing point 54 58 DEG C, be one be widely used in Cotton Gossypii, Semen Maydis,
The selectivity soil of Oryza sativa L., Rhizoma Solani tuber osi, Semen sojae atricolor, Semen arachidis hypogaeae, Nicotiana tabacum L. and vegetable fields closes weeding
Agent.Pendimethalin is inner sucting conduction type selective herbicide, but its conductive performance is poor.It
Have no effect on the sprouting of weed seed, but plumelet, stem and root during suppressing weed seed germination
Work after absorbing medicament.Pendimethalin applied range, drug effect is preferable, is difficult to cause
Poisoning.Be applicable to Semen sojae atricolor, Semen Maydis, Semen arachidis hypogaeae, Semen Pisi sativi, Cotton Gossypii, Herba Apii graveolentis, Nicotiana tabacum L., Helianthi,
Oryza sativa L., various vegetables and orchard are prevented and kill off barnyard grass, Herba Digitariae, Herba Setariae Viridis, multitude, Herba Amaranthi tricoloris etc. annual
Weeds.Many countries such as the U.S., Europe, Japan, Israel, India, Australia and ground
District spread already uses, and what product mainly had that BASF AG produces 33% executes field and mend newborn
Oil etc..The active component of dinitroaniline has stronger colorability, cream, suspending agent
Serious coloring would generally be caused Deng liquid preparation, in use affect operator, pollute
Application equipment.
Patent US4871392 mentions that in its background technology Pendimethalin exists with polymorphic.
Polymorph crystals may cause fusing point to reduce, when it is prepared as suspending agent, at high temperature ripple
In the case of Dong, the form of Pendimethalin converts between solid, liquid, in temperature
Time higher, existing with liquid condition, temperature reverts to solid when reducing, and has in this process
The crystal of substantial amounts of coarse-grain form occurs, this will cause suspending agent physical stability to be destroyed.For
Solution the problems referred to above, are feasible solutions by its microencapsulation.The preparation side of microcapsule
Method is broadly divided into 3 classes: polyreaction method, phase separation method, physics and Mechanical Method.Polymerization is anti-
Method is answered to include interfacial polymerization, situ aggregation method and suspension colloid connection method；Phase separation method includes aqueous phase
Phase separation method and oil phase phase separation method；Physics and Mechanical Method include fusing dispersion condensation method, spraying
Seasoning, solvent or solution extraction etc..But feature based on the former medicine of Pendimethalin, by passing
System method is prepared as microcapsule suspending agent and there is the biggest difficulty, the especially system of high-load
Agent, such as 400g/L-450g/L Pendimethalin microcapsule suspending agent, enough molten because adding
Agent, Pendimethalin still suffers from above-mentioned along with the change of ambient temperature in the system of microencapsulation
Solid, the transformation of liquid form, in long term storage, preparation system is easily broken,
Cause solidification or gradually solidify during long-term storage；Patent CN102770023A carries
Gone out to utilize alkali salt, alkali metal salt to solve this problem, and a large amount of alkali metal salt,
Alkali salt is disadvantageous to the long term storage stability of suspension system.
Summary of the invention
For defect present in prior art, it is an object of the invention to provide a kind of diformazan penta
Happy spirit microcapsule suspending agent and preparation method thereof, the method uses polyureas or poly-by interfacial polymerization
Urethane is as cyst wall, and Pendimethalin, as capsule-core, selects suitable emulsifying agent, dispersant etc.
Prepare Pendimethalin microcapsule suspending agent, overcome the defect of cream and suspending agent, solve simultaneously
Liquid preparation easy coloring, contaminated equipment, the problem that affects user.
For reaching object above, the present invention adopts the technical scheme that:
The present invention provides a kind of Pendimethalin microcapsule suspending agent,
The microcapsule capsule-core (or effective ingredient) of described Pendimethalin microcapsule suspending agent is diformazan penta
Happy spirit, in described Pendimethalin microcapsule suspending agent, content is 10 450g/L；
The microcapsule wall of described Pendimethalin microcapsule suspending agent is polyureas or polyurethane, described
In Pendimethalin microcapsule suspending agent, content is 20 100g/L；
Possibly together with emulsifying agent 20 100g/L, dispersion in described Pendimethalin microcapsule suspending agent
Agent 20 60g/L, antifreezing agent 30 100g/L, viscosity modifier 1 10g/L and defoamer
2 15g/L, surplus is water；Described water is the solvent of described Pendimethalin microcapsule suspending agent.
In above-mentioned Pendimethalin microcapsule suspending agent, possibly together with preservative 1 5g/L.
In above-mentioned Pendimethalin microcapsule suspending agent, described polyureas is different by cyst material monomer
Cyanate and cyst material monomeric polycarboxylic amine are preparing described Pendimethalin microcapsule suspending agent mistake
Journey generates through polycondensation reaction；
Described polyurethane is by cyst material monomeric diisocyanate and cyst material monomeric polyols
Generate through polycondensation reaction during preparing described Pendimethalin microcapsule suspending agent；
In above-mentioned Pendimethalin microcapsule suspending agent, described isocyanates can be toluene diisocyanate
In acid esters, methyl diphenylene diisocyanate and poly methylene poly phenyl poly isocyanate at least
A kind of；
Described polyamine be ethylenediamine, hexamethylene diamine, propane diamine, p-phenylenediamine, triethanolamine,
At least one in diethyl amino propylamine and diethylenetriamine；
Described polyhydric alcohol be ethylene glycol, glycerol, diglycol, trimethylolpropane and
At least one in tetramethylolmethane.
In above-mentioned Pendimethalin microcapsule suspending agent, described emulsifying agent is alkylphenol-polyethenoxy
Ether (such as OP-10), fatty alcohol-polyoxyethylene ether are (such as AEO-10, AEO-9, AEO-8, AEO-13
Or AEO-7) at least one.
In above-mentioned Pendimethalin microcapsule suspending agent, described dispersant is naphthalene sulphonate formaldehyde contracting
Compound (concretely alkylnaphthalene sulfonate formaldehyde condensation products such as Morwet D-425), fatty alcohol
Polyoxyethylene ether phosphate (such as Dispersogen LFS), EO-PO block copolymer (as
Emulsogen 3510), sodium lignin sulfonate (such as Polyfon F), styryl phenol polyoxy
Ethylene polyethenoxy ether, alkyl naphthalene formaldehyde condensation substance sodium sulfonate, the graft copolymerization of macromolecule pectination
Thing (such as polymeric acrylic acid family macromolecule graft copolymer Tersperse 2500), phosphate ester
In class dispersant (such as Soprophor SC), inorganic salt dispersants and polymerization of carboxylic acid salt at least
A kind of.
In above-mentioned Pendimethalin microcapsule suspending agent, described antifreezing agent be ethylene glycol, propylene glycol,
At least one in glycerol and carbamide；
Described viscosity modifier is at least one in xanthan gum, Polyethylene Glycol and polyvinyl alcohol；
Described preservative is sodium benzoate and isothiazolinone preservative (such as isothiazolone)
In at least one；
Described defoamer be organic silicon defoamer (such as SAG1522) and polyether antifoam agent (as
B-299) at least one in；
Described water is deionized water and/or distilled water.
In above-mentioned Pendimethalin microcapsule suspending agent, described Pendimethalin microcapsule suspending agent
Median D50It is 5～10 μm；And/or D90It is 6～11 μm.
Present invention also offers the preparation method of described Pendimethalin microcapsule suspending agent, including such as
Lower step:
The former medicine of described Pendimethalin is heated to molten condition by a, adds described cyst material
Monomeric diisocyanate, stirs, and adds described emulsifying agent, is uniformly mixing to obtain oil phase；
B is sequentially added into described cyst material monomeric polycarboxylic amine or polyhydric alcohol, described antifreeze in water
Agent, the described dispersant of half quality and described defoamer, be uniformly mixing to obtain aqueous phase；
After described oil phase and described aqueous phase are mixed by c, obtain O/w emulsion；Specifically, will
After described oil phase and the mixing of described aqueous phase, in 5000 10000rpm down cut emulsifyings 1.5
3min, obtains O/w emulsion；
Described O/w emulsion is incubated under 60～70 DEG C of water-baths by d, and stirs to having reacted
After complete (i.e. cyst wall and capsule-core is completely formed microcapsule), stop insulation, natural under agitation
It is cooled to room temperature, adds the described dispersant of second half quality and described viscosity modifier, stir
Mix uniformly, it is thus achieved that described Pendimethalin microcapsule suspending agent.
In step c and step d, after described oil phase and described aqueous phase are mixed, in oil phase
Described cyst material monomeric polycarboxylic amine in described cyst material monomeric diisocyanate and aqueous phase or
Polyhydric alcohol generation polycondensation reaction, forms microcapsule wall polyureas or polyurethane, by Pendimethalin bag
It is rolled in microcapsule capsule-core.
In above-mentioned preparation method, in step d, when adding described viscosity modifier, also wrap
Include the step adding described preservative.
In above-mentioned preparation method, step a and b are carried out at 60～70 DEG C, the response time
Can be adjusted according to equipment with stir speed (S.S.)；
And/or, in step c, the median D of described O/w emulsion50It is 4 μm～7 μm；
And/or, in step d, the speed of the described stirring in described stirring to reaction completely is
100 500rpm, the time of described reaction is 2 3h；
And/or, the preparation method of described Pendimethalin microcapsule suspending agent is entered in atmospheric conditions
OK；
And/or, the preparation method of described Pendimethalin microcapsule suspending agent does not include adding alkaline earth
Metal and/or alkali metal salt compounds and/or the step of catalyst.
In above-mentioned preparation method, when preparing every liter of described Pendimethalin microcapsule suspending agent:
In step a, (effective ingredient) Han Pendimethalin in the former medicine of described Pendimethalin
It is 10 450g (such as 10g, 50g, 100g, 330g, 400g, 450g), described Carbimide.
Ester consumption is 10 90g (such as 10g, 90g, 30g, 50g, 40g), described emulsifier
It is 20 100g (such as 100g, 20g, 30g, 50g)；
In step b, described polyamine consumption is 10 50g (such as 10g, 30g, 50g), institute
Stating polyhydric alcohol consumption is 10 50g (such as 10g, 50g), the described dispersion of described half quality
Agent is 10 30g (such as 30g, 25g, 20g, 15g, 10g)；Described antifreezing agent consumption is
30 100 (such as 30g, 50g, 80g, 100g)；Described defoamer consumption be 2 15g (as
2g、5g、6g、8g、10g、15g)；
In step d, the described dispersant of second half quality described be 10 30g (as 30g,
25g、20g、15g、10g)；Described viscosity modifier consumption be 1 10g (as 1g, 2g,
5g、10g)；Described preservative consumption is 1 5g (such as 1g, 2g, 5g).
The invention have the advantages that
The present invention solves liquid preparation easily by the Pendimethalin microcapsule suspending agent of preparation
Color, the problem polluting application equipment；Without solvent in preparation, environmentally friendly；Solve low
Melting point compounds is easily generated, with temperature fluctuation, the problem that coarse crystal causes system livering；By using
Suitably dispersant and emulsifying agent, adds a small amount of (half during preparing O/w emulsion
Consumption) dispersant, do not use a large amount of alkaline-earth metal, alkaline metal salt, after both can preventing encystation
Microcapsule assemble, also improve the long term storage stability of product；The dispersant that the present invention uses
With the problem that emulsifier combination can solve microcapsule suspending agent solidification, having of high-load can be prepared
The Pendimethalin microcapsule suspending agent of long term storage stability；The present invention has carried out temperature control,
Changing into carrying out under normal pressure, be not required to use catalyst, process is simple, it is not necessary to special installation, becomes
This is cheap.
Detailed description of the invention
Experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., if no special instructions, all can be from business
Approach obtains.
% in following embodiment is weight/mass percentage composition if no special instructions.
Can be according to the volume of production Pendimethalin microcapsule suspending agent in actual production, by following
The each amounts of components producing 1L Pendimethalin microcapsule suspending agent in Example formulations carries out geometric ratio
Example zooms in or out.
Reagent used in following embodiment is specific as follows:
The former medicine of Pendimethalin, active constituent content 97%, manufacturer: Yongan, Lianshui chemical industry
Company limited；
Toluene di-isocyanate(TDI) (cyst material monomer), purity is 99%, manufacturer: on
Sea Bayer polyurethane company limited；
Methyl diphenylene diisocyanate (cyst material monomer), purity is 99%, factory
Shanghai Bayer polyurethane company limited of family；
Poly methylene poly phenyl poly isocyanate (cyst material monomer), purity is 99%, raw
Product producer: Shanghai Basf Polyurethane Co., Ltd.；
AEO-10 (fatty alcohol-polyoxyethylene ether, emulsifying agent), manufacturer: Hai'an oil
Work company limited；
AEO-9 (fatty alcohol-polyoxyethylene ether, emulsifying agent), manufacturer: Hai'an petrochemical industry
Company limited；
AEO-8 (fatty alcohol-polyoxyethylene ether, emulsifying agent), manufacturer: Hai'an petrochemical industry
Company limited；
AEO-13 (fatty alcohol-polyoxyethylene ether, emulsifying agent), manufacturer: Hai'an petrochemical industry
Company limited；
AEO-7 (fatty alcohol-polyoxyethylene ether, emulsifying agent), manufacturer: Hai'an petrochemical industry
Company limited；
OP-10 (alkylphenol polyoxyethylene, emulsifying agent), manufacturer: Luo Diya group；
Ethylenediamine (cyst material monomer), manufacturer: BASF Auxiliary Chemicals Co., Ltd.；
Tetramethylolmethane (cyst material monomer), manufacturer: the limited public affairs of BASF application chemical industry
Department；
Diethyl amino propylamine (cyst material monomer), manufacturer: BASF application chemical industry has
Limit company；
P-phenylenediamine (cyst material monomer), manufacturer: the limited public affairs of BASF application chemical industry
Department；
Glycerol (cyst material monomer) manufacturer: BASF Auxiliary Chemicals Co., Ltd.；
Morwet D-425 (alkylnaphthalene sulfonate formaldehyde condensation products, dispersant), manufacturer:
Akzo Nobel company limited；
Emulsogen 3510 (EO-PO block copolymer, dispersant), manufacturer: section
Lai En Chemical Co., Ltd.；
Tersperse 2500 (polymeric acrylic acid family macromolecule graft copolymer, dispersant),
Manufacturer: the graceful group of Hensel；
Polyfon F (sodium lignin sulfonate, dispersant), manufacturer: the real big gram of chemistry of dimension
Product company limited；
Soprophor SC (phosphoric acid ester dispersant), manufacturer: Luo Diya group；
Dispersogen LFS (aliphatic alcohol polyoxyvinethene phosphate), manufacturer: section's Lay
Grace Chemical Co., Ltd.；
Glycerol (antifreezing agent), manufacturer: BASF Auxiliary Chemicals Co., Ltd.；
Carbamide (antifreezing agent), manufacturer: BASF Auxiliary Chemicals Co., Ltd.；
Ethylene glycol (antifreezing agent), manufacturer: BASF Auxiliary Chemicals Co., Ltd.；
Propylene glycol (antifreezing agent), manufacturer: BASF Auxiliary Chemicals Co., Ltd.；
SAG 1522 (organic silicon defoamer), manufacturer: Mai Tu new high-tech material company limited；
B-299 (polyether antifoam agent), manufacturer: middle federal Fine Chemical Co., Ltd；
Xanthan gum (viscosity modifier), manufacturer: Luo Diya group；
Polyvinyl alcohol (viscosity modifier), manufacturer: Kuraray international trade (Shanghai)
Company limited；
Polyethylene Glycol (viscosity modifier), PEG8000, manufacturer: DOW Chemical is limited
Company；
Isothiazolone (preservative), manufacturer: Clariant Chemical Co., Ltd.；
Sodium benzoate (preservative), manufacturer: magnificent hundred million chemical industry Industrial Co., Ltd.s.
Embodiment 1,10g/L Pendimethalin microcapsule suspending agent
According to the consumption of table 1, it is heated to melting by former for Pendimethalin medicine (effective ingredient 10g)
Melt state, add 10g toluene di-isocyanate(TDI) (cyst material monomer), after stirring again
Add 100g AEO-10 (emulsifying agent), three's mix homogeneously is prepared as oil phase；
10g ethylenediamine (cyst material monomer), 50g glycerol it is sequentially added in distilled water
(antifreezing agent), 30g Morwet D-425 (dispersant) and 15g SAG 1522 (defoamer),
Stir and be prepared as aqueous phase；
It is incubated oil phase respectively with aqueous phase to prevent Pendimethalin former under 60 DEG C of waters bath with thermostatic control
Medicine is met cold analysis and is gone out, after oil phase and aqueous phase being mixed, at 10000rpm down cut emulsifying 1.5min
(D50Control in 5 μm～7 μm), prepare O/w emulsion；
It is incubated to prevent Pendimethalin under 60 DEG C of water-baths by the O/w emulsion prepared
Former medicine is met cold analysis and is gone out, and reacts 2.5h, make cyst wall whole with capsule-core under 500rpm stirring condition
Form microcapsule；
Stop insulation, naturally cool to room temperature under agitation.Add 250g 2% xanthan gum
(viscosity modifier) aqueous solution (containing 2% isothiazolone (preservative)), 30g Morwet D-425
(dispersant), is uniformly mixing to obtain finished product: 10g/L Pendimethalin microcapsule suspending agent, i.e.
The microcapsule capsule-core of described Pendimethalin microcapsule suspending agent is Pendimethalin, at described diformazan penta
In happy spirit microcapsule suspending agent, content is 10g/L；The microcapsule of described Pendimethalin microcapsule suspending agent
Cyst wall is polyureas, and in described Pendimethalin microcapsule suspending agent, content is 20g/L.
The testing result such as table 2 of the 10g/L Pendimethalin microcapsule suspending agent that the present embodiment prepares
Shown in.As shown in Table 2, the present embodiment can obtain physical property and stable chemical performance, bag
The Pendimethalin microcapsule suspending agent that envelope rate is high, in use, not contaminated equipment and spraying
Region, does not affect user.
The formula of table 1. 10g/L Pendimethalin microcapsule suspending agent
The testing result of table 2. 10g/L Pendimethalin microcapsule suspending agent
Note: the assay method of the envelop rate in table 2 and other table of the present invention is as follows: accurately draw
1ml finished product collected after centrifugation supernatant, and it is settled to 100ml with 0.1mol/L hydrochloric acid, with
0.1mol/L hydrochloric acid is blank, and ultraviolet spectrophotometer measures absorbance, according to as follows
Formula II calculating Pendimethalin envelop rate (%):
Embodiment 2. 50g/L Pendimethalin microcapsule suspending agent
According to the consumption of table 3, it is heated to melting by former for Pendimethalin medicine (effective ingredient 50g)
Melting state, add 90g methyl diphenylene diisocyanate (cyst material monomer), stirring is all
Add 20g OP-10 after even, three's mix homogeneously is prepared as oil phase；
It is sequentially added into 10g tetramethylolmethane (cyst material monomer), 50g urine in deionized water
Element (antifreezing agent), 20g Emulsogen 3510 (dispersant) and 10g polyether antifoam agent (disappear
Infusion), stir and be prepared as aqueous phase；
Oil phase is incubated respectively with aqueous phase under 60 DEG C of waters bath with thermostatic control, after oil phase and aqueous phase are mixed,
At 5000rpm down cut emulsifying 2.5min (D50Control in 4 μm～7 μm), prepare water
Bag fat liquor；
The O/w emulsion prepared is incubated under 60 DEG C of water-baths, stirs bar at 500rpm
React 2h under part, make cyst wall and capsule-core be completely formed microcapsule；
Stop insulation, naturally cool to room temperature under agitation.Add 50g 2% xanthan gum
(viscosity modifier) aqueous solution (containing 2% sodium benzoate (preservative)) and 20g Emulsogen
3510 (dispersants), are uniformly mixing to obtain finished product: 50g/L Pendimethalin microcapsule suspending agent,
The microcapsule capsule-core of the most described Pendimethalin microcapsule suspending agent is Pendimethalin, at described diformazan
In penta happy spirit microcapsule suspending agent, content is 50g/L；Described Pendimethalin microcapsule suspending agent micro-
Capsule cyst wall is polyurethane, and in described Pendimethalin microcapsule suspending agent, content is 100g/L.
The testing result such as table 4 of the 50g/L Pendimethalin microcapsule suspending agent that the present embodiment prepares
Shown in.As shown in Table 4, the present embodiment can obtain physical property and stable chemical performance, bag
The Pendimethalin microcapsule suspending agent that envelope rate is high, in use, not contaminated equipment and spraying
Region, does not affect user.
The formula of table 3. 50g/L Pendimethalin microcapsule suspending agent
| Function | Component | Consumption, g |
| Effective ingredient (capsule-core) | The former medicine of Pendimethalin (folding hundred) | 50 |
| Emulsifying agent | OP-10 (alkylphenol polyoxyethylene) | 20 |
| Cyst material monomer | Methyl diphenylene diisocyanate | 90 |
| Cyst material monomer | Tetramethylolmethane | 10 |
| Dispersant | Emulsogen 3510 (EO-PO block copolymer) | 40 |
| Antifreezing agent | Carbamide | 50 |
| Viscosity modifier | Xanthan gum | 1 |
| Preservative | Sodium benzoate | 1 |
| Defoamer | Polyether antifoam agent | 10 |
| Diluent | Deionized water | Complement to 1L |
Table 4. 50g/L Pendimethalin microcapsule suspending agent testing result
Embodiment 3. 100g/L Pendimethalin microcapsule suspending agent
According to the consumption of table 5, former for Pendimethalin medicine (effective ingredient 100g) is heated to
Molten condition, adds 30g methyl diphenylene diisocyanate (cyst material monomer), stirring
Add 50g AEO-9 (emulsifying agent) after Jun Yun, three's mix homogeneously is prepared as oil phase；
It is sequentially added into 30g diethyl amino propylamine (cyst material monomer), 80g in deionized water
Glycerol (antifreezing agent), 25g Dispersogen LFS (dispersant) and 8g organosilicon
Defoamer (defoamer), stirs and is prepared as aqueous phase；
Oil phase is incubated respectively with aqueous phase under 60 DEG C of waters bath with thermostatic control, after oil phase and aqueous phase are mixed,
At 8000rpm down cut emulsifying 2min (D50Control in 5 μm～7 μm), prepare water bag
Fat liquor；
The O/w emulsion prepared is incubated under 60 DEG C of water-baths, stirs bar at 500rpm
React 2h under part, make cyst wall and capsule-core be completely formed microcapsule；
Stop insulation, naturally cool to room temperature under agitation.Add the poly-second of 50g 10%
Enolate solution and 25g Dispersogen LFS, be uniformly mixing to obtain finished product: 100g/L bis-
First penta happy spirit microcapsule suspending agent, the microcapsule capsule-core of the most described Pendimethalin microcapsule suspending agent is two
The happy spirit of first penta, in described Pendimethalin microcapsule suspending agent, content is 100g/L；Described two
The microcapsule wall of first penta happy spirit microcapsule suspending agent is polyureas, at described Pendimethalin microcapsule suspension
In agent, content is 60g/L.
The testing result such as table of the 100g/L Pendimethalin microcapsule suspending agent that the present embodiment prepares
Shown in 6.As shown in Table 6, the present embodiment can obtain physical property and stable chemical performance,
The Pendimethalin microcapsule suspending agent that envelop rate is high, in use, not contaminated equipment and spray
Execute region, user is not affected.
The formula of table 5. 100g/L Pendimethalin microcapsule suspending agent
Table 6. 100g/L Pendimethalin suspending agent testing result
Embodiment 4. 330g/L Pendimethalin microcapsule suspending agent
According to the consumption of table 7, former for Pendimethalin medicine (effective ingredient 330g) is heated to
Molten condition, adds 50g methyl diphenylene diisocyanate (cyst material monomer), stirring
Add 100g AEO-8 (emulsifying agent) after Jun Yun, three's mix homogeneously is prepared as oil phase；
It is sequentially added into 30g diethyl amino propylamine (cyst material monomer), 100g in deionized water
Glycerol (antifreezing agent), 10g Tersperse 2500 (dispersant) and 6g organosilicon disappear
Infusion (defoamer), stirs and is prepared as aqueous phase；
Oil phase is incubated respectively with aqueous phase under 70 DEG C of waters bath with thermostatic control, after oil phase and aqueous phase are mixed,
At 8000rpm down cut emulsifying 2min (D50Control in 5 μm～7 μm), prepare water bag
Fat liquor；
The O/w emulsion prepared is incubated under 70 DEG C of water-baths, stirs bar at 300rpm
React 2h under part, make cyst wall and capsule-core be completely formed microcapsule；
Stop insulation, naturally cool to room temperature under agitation.Add the poly-second of 100g 10%
Glycol (viscosity modifier) aqueous solution and 10g Tersperse 2500 (dispersant), stirring
Uniformly obtain finished product: 330g/L Pendimethalin microcapsule suspending agent, the most described Pendimethalin is micro-
The microcapsule capsule-core of capsule suspending agent is Pendimethalin, in described Pendimethalin microcapsule suspending agent
Content is 330g/L；The microcapsule wall of described Pendimethalin microcapsule suspending agent is polyureas,
In described Pendimethalin microcapsule suspending agent, content is 80g/L.
The testing result such as table of the 330g/L Pendimethalin microcapsule suspending agent that the present embodiment prepares
Shown in 8.As shown in Table 8, the present embodiment can obtain physical property and stable chemical performance,
The Pendimethalin microcapsule suspending agent that envelop rate is high, in use, not contaminated equipment and spray
Execute region, user is not affected.
The formula of table 7. 330g/L Pendimethalin microcapsule suspending agent
Table 8. 330g/L Pendimethalin microcapsule suspending agent testing result
Embodiment 5. 400g/L Pendimethalin microcapsule suspending agent
According to the consumption of table 9, former for Pendimethalin medicine (effective ingredient 400g) is heated to
Molten condition, adds 50g poly methylene poly phenyl poly isocyanate (cyst material monomer),
Add 20g AEO-13 (emulsifying agent) after stirring, three's mix homogeneously is prepared as oil
Phase；
20g p-phenylenediamine (cyst material monomer), 30g second two it is sequentially added in distilled water
Alcohol (antifreezing agent), 15g Polyfon F (sodium lignin sulfonate, dispersant) and 2g have
Machine silicon defoaming agent (defoamer), stirs and is prepared as aqueous phase；
Oil phase is incubated respectively with aqueous phase under 65 DEG C of waters bath with thermostatic control, after oil phase and aqueous phase are mixed,
At 6000rpm down cut emulsifying 3min (D50Control in 6 μm～7 μm), prepare water bag
Fat liquor；
The O/w emulsion prepared is incubated under 65 DEG C of water-baths, stirs bar at 400rpm
React 2h under part, make cyst wall and capsule-core be completely formed microcapsule；
Stop insulation, naturally cool to room temperature under agitation.Add 50g 2% xanthan gum
Aqueous solution (containing 2% isothiazolone), 15g Polyfon F (sodium lignin sulfonate),
It is uniformly mixing to obtain finished product: 400g/L Pendimethalin microcapsule suspending agent, the most described diformazan penta
The microcapsule capsule-core of happy spirit microcapsule suspending agent is Pendimethalin, hangs at described Pendimethalin microcapsule
In floating agent, content is 400g/L；The microcapsule wall of described Pendimethalin microcapsule suspending agent is poly-
Urea, in described Pendimethalin microcapsule suspending agent, content is 100g/L.
The testing result such as table of the 400g/L Pendimethalin microcapsule suspending agent that the present embodiment prepares
Shown in 10.As shown in Table 10, the present embodiment can obtain physical property and stable chemical performance,
The Pendimethalin microcapsule suspending agent that envelop rate is high, in use, not contaminated equipment and spray
Execute region, user is not affected.
The formula of table 9. 400g/L Pendimethalin microcapsule suspending agent
| Function | Component | Consumption, g |
| Effective ingredient (capsule-core) | The former medicine of Pendimethalin (folding hundred) | 400 |
| Emulsifying agent | AEO-13 (fatty alcohol-polyoxyethylene ether) | 20 |
| Cyst material monomer | Poly methylene poly phenyl poly isocyanate | 50 |
| Cyst material monomer | P-phenylenediamine | 50 |
| Dispersant | Polyfon F (sodium lignin sulfonate) | 30 |
| Antifreezing agent | Ethylene glycol | 30 |
| Viscosity modifier | Xanthan gum | 1 |
| Preservative | Isothiazolone | 1 |
| Defoamer | Organic silicon defoamer | 2 |
| Diluent | Distilled water | Complement to 1L |
Table 10. 400g/L Pendimethalin microcapsule suspending agent testing result
Embodiment 6. 450g/L Pendimethalin microcapsule suspending agent
According to the consumption of table 11, former for Pendimethalin medicine (effective ingredient 450g) is heated to
Molten condition, adds 40g poly methylene poly phenyl poly isocyanate (cyst material monomer),
Add 30g AEO-7 (emulsifying agent) after stirring, three's mix homogeneously is prepared as oil
Phase；
It is sequentially added into 50g glycerol (cyst material monomer), 50g the third two in deionized water
Alcohol (antifreezing agent), 15g Soprophor SC (phosphate ester) (dispersant) and 5g are organic
Silicon defoaming agent (defoamer), stirs and is prepared as aqueous phase；
Oil phase is incubated respectively with aqueous phase under 65 DEG C of waters bath with thermostatic control, after oil phase and aqueous phase are mixed,
At 8000rpm down cut emulsifying 3min (D50Control in 5 μm～7 μm), prepare water bag
Fat liquor；
The O/w emulsion prepared is incubated under 65 DEG C of water-baths, stirs bar at 450rpm
React 3h under part, make cyst wall and capsule-core be completely formed microcapsule；
Stop insulation, naturally cool to room temperature under agitation.Add 100g 2% xanthan gum
(viscosity modifier) aqueous solution (containing 2% isothiazolone), 15g Soprophor SC (phosphorus
Acid esters) (dispersant), it is uniformly mixing to obtain finished product: 450g/L Pendimethalin microcapsule suspension
Agent, the microcapsule capsule-core of the most described Pendimethalin microcapsule suspending agent is Pendimethalin, described
In Pendimethalin microcapsule suspending agent, content is 450g/L；Described Pendimethalin microcapsule suspension
The microcapsule wall of agent is polyurethane, and in described Pendimethalin microcapsule suspending agent, content is
90g/L。
The testing result such as table of the 450g/L Pendimethalin microcapsule suspending agent that the present embodiment prepares
Shown in 12.As shown in Table 12, the present embodiment can obtain physical property and stable chemical performance,
The Pendimethalin microcapsule suspending agent that envelop rate is high, in use, not contaminated equipment and spray
Execute region, user is not affected.
The formula of table 11. 450g/L Pendimethalin microcapsule suspending agent
| Function | Component | Consumption, g |
| Effective ingredient (capsule-core) | The former medicine of Pendimethalin (folding hundred) | 450 |
| Emulsifying agent | AEO-7 (fatty alcohol-polyoxyethylene ether) | 30 |
| Cyst material monomer | Poly methylene poly phenyl poly isocyanate | 40 |
| Cyst material monomer | Glycerol | 50 |
| Dispersant | Soprophor SC (phosphoric acid ester dispersant) | 30 |
| Antifreezing agent | Propylene glycol | 50 |
| Viscosity modifier | Xanthan gum | 2 |
| Preservative | Isothiazolone | 2 |
| Defoamer | Organic silicon defoamer | 5 |
| Diluent | Deionized water | Complement to 1L |
Table 12. 450g/L Pendimethalin microcapsule suspending agent testing result
The content not being described in detail in this specification belongs to known in professional and technical personnel in the field
Prior art.
Claims (10)
1. a Pendimethalin microcapsule suspending agent, it is characterised in that
The microcapsule capsule-core of described Pendimethalin microcapsule suspending agent is Pendimethalin, described two
In first penta happy spirit microcapsule suspending agent, content is 10 450g/L；
The microcapsule wall of described Pendimethalin microcapsule suspending agent is polyureas or polyurethane, described
In Pendimethalin microcapsule suspending agent, content is 20 100g/L；
Possibly together with emulsifying agent 20 100g/L, dispersion in described Pendimethalin microcapsule suspending agent
Agent 20 60g/L, antifreezing agent 30 100g/L, viscosity modifier 1 10g/L and defoamer
2 15g/L, surplus is water.
2. Pendimethalin microcapsule suspending agent as claimed in claim 1, it is characterised in that
Possibly together with preservative 1 5g/L in described Pendimethalin microcapsule suspending agent.
3. Pendimethalin microcapsule suspending agent as claimed in claim 1 or 2, it is characterised in that
Described polyureas is to be prepared by cyst material monomeric diisocyanate and cyst material monomeric polycarboxylic amine
Generate through polycondensation reaction during described Pendimethalin microcapsule suspending agent；
Described polyurethane is by cyst material monomeric diisocyanate and cyst material monomeric polyols
Generate through polycondensation reaction during preparing described Pendimethalin microcapsule suspending agent.
4. Pendimethalin microcapsule suspending agent as claimed in claim 3, it is characterised in that
Described isocyanates is toluene di-isocyanate(TDI), methyl diphenylene diisocyanate and Duo Ya
At least one in methyl polyphenyl polyisocyanate；
Described polyamine be ethylenediamine, hexamethylene diamine, propane diamine, p-phenylenediamine, triethanolamine,
At least one in diethyl amino propylamine and diethylenetriamine；
Described polyhydric alcohol be ethylene glycol, glycerol, diglycol, trimethylolpropane and
At least one in tetramethylolmethane.
5. Pendimethalin microcapsule suspending agent as claimed in claim 1 or 2, it is characterised in that
Described emulsifying agent is at least in alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether
Kind；
Described dispersant be naphthalenesulfonate formaldehyde condensation compound, aliphatic alcohol polyoxyvinethene phosphate,
EO-PO block copolymer, sodium lignin sulfonate, styryl phenol polyethenoxy polyethenoxy ether,
Alkyl naphthalene formaldehyde condensation substance sodium sulfonate, the graft copolymer of macromolecule pectination, phosphoric acid ester disperse
At least one in agent, inorganic salt dispersants and polymerization of carboxylic acid salt.
6. Pendimethalin microcapsule suspending agent as claimed in claim 1 or 2, it is characterised in that
Described antifreezing agent is at least one in ethylene glycol, propylene glycol, glycerol and carbamide；
Described viscosity modifier is at least one in xanthan gum, Polyethylene Glycol and polyvinyl alcohol；
Described preservative is sodium benzoate and isothiazolinone at least one of the preservatives；
Described defoamer is at least one in organic silicon defoamer and polyether antifoam agent；
Described water is deionized water and/or distilled water.
7. Pendimethalin microcapsule suspending agent as claimed in claim 1 or 2, it is characterised in that
The median D of described Pendimethalin microcapsule suspending agent50It is 5～10 μm.
8. the preparation side of arbitrary described Pendimethalin microcapsule suspending agent in claim 17
Method, comprises the steps:
The former medicine of described Pendimethalin is heated to molten condition by a, adds described cyst material
Monomeric diisocyanate, stirs, and adds described emulsifying agent, is uniformly mixing to obtain oil phase；
B is sequentially added into described cyst material monomeric polycarboxylic amine or polyhydric alcohol, described antifreeze in water
Agent, the described dispersant of half quality and described defoamer, be uniformly mixing to obtain aqueous phase；
After described oil phase and described aqueous phase are mixed by c, obtain O/w emulsion；
Described O/w emulsion is incubated under 60～70 DEG C of water-baths by d, and stirs to reaction completely
After, stop insulation, naturally cool to room temperature under agitation, add the institute of second half quality
State dispersant and described viscosity modifier, it is thus achieved that described Pendimethalin microcapsule suspending agent.
9. the preparation method of Pendimethalin microcapsule suspending agent as claimed in claim 8, it is special
Levy and be, in step d, when adding described viscosity modifier, also include adding described anticorrosion
The step of agent.
10. the preparation method of Pendimethalin microcapsule suspending agent as described in claim 8 or 9,
It is characterized in that,
Step a and b are carried out at 60～70 DEG C；
And/or, in step c, the median D of described O/w emulsion50It is 4 μm～7 μm；
And/or, in step d, the speed of the described stirring in described stirring to reaction completely is
100 500rpm, the time of described reaction is 2 3h；
And/or, the preparation method of described Pendimethalin microcapsule suspending agent is entered in atmospheric conditions
OK；
And/or, the preparation method of described Pendimethalin microcapsule suspending agent does not include adding alkaline earth
Metal and/or alkali metal salt compounds and/or the step of catalyst.
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| CN107094761A (en) * | 2017-06-12 | 2017-08-29 | 南京高正农用化工有限公司 | A kind of Pendimethalin microcapsule suspending agent and preparation method thereof |
| CN108353897A (en) * | 2018-03-27 | 2018-08-03 | 江苏精禾界面科技有限公司 | A kind of pesticide microcapsule suspending agent and preparation method thereof |
| CN108378027A (en) * | 2018-03-20 | 2018-08-10 | 南京高正农用化工有限公司 | A kind of microcapsule suspension-suspendinagent agent containing Pendimethalin and flumioxazin |
| CN108552170A (en) * | 2018-03-27 | 2018-09-21 | 江苏精禾界面科技有限公司 | A kind of Pendimethalin microcapsules and its high efficiency preparation method |
| CN108782549A (en) * | 2018-07-17 | 2018-11-13 | 郭秦 | A kind of compounding low melting point suspending agent technique |
| CN111109251A (en) * | 2019-12-18 | 2020-05-08 | 中化化工科学技术研究总院有限公司 | Wetting dispersant and pendimethalin suspending agent using same |
| CN111972422A (en) * | 2019-05-21 | 2020-11-24 | 江苏龙灯化学有限公司 | Weeding composition containing microcapsules and preparation method and application thereof |
| CN114246182A (en) * | 2021-12-30 | 2022-03-29 | 江苏仁信作物保护技术有限公司 | Pendimethalin microcapsule suspending agent and production process thereof |
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| CN112042646B (en) * | 2020-09-09 | 2022-09-30 | 中农立华生物科技股份有限公司 | Pendimethalin suspending agent and low-energy-consumption preparation method thereof |
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| CN107094761A (en) * | 2017-06-12 | 2017-08-29 | 南京高正农用化工有限公司 | A kind of Pendimethalin microcapsule suspending agent and preparation method thereof |
| CN107094761B (en) * | 2017-06-12 | 2018-06-22 | 南京高正农用化工有限公司 | A kind of Pendimethalin microcapsule suspending agent and preparation method thereof |
| CN108378027A (en) * | 2018-03-20 | 2018-08-10 | 南京高正农用化工有限公司 | A kind of microcapsule suspension-suspendinagent agent containing Pendimethalin and flumioxazin |
| CN108353897A (en) * | 2018-03-27 | 2018-08-03 | 江苏精禾界面科技有限公司 | A kind of pesticide microcapsule suspending agent and preparation method thereof |
| CN108552170A (en) * | 2018-03-27 | 2018-09-21 | 江苏精禾界面科技有限公司 | A kind of Pendimethalin microcapsules and its high efficiency preparation method |
| CN108552170B (en) * | 2018-03-27 | 2021-01-12 | 江苏精禾界面科技有限公司 | Pendimethalin microcapsule and efficient preparation method thereof |
| CN108353897B (en) * | 2018-03-27 | 2021-03-16 | 江苏精禾界面科技有限公司 | Pesticide microcapsule suspending agent and preparation method thereof |
| CN108782549A (en) * | 2018-07-17 | 2018-11-13 | 郭秦 | A kind of compounding low melting point suspending agent technique |
| CN111972422A (en) * | 2019-05-21 | 2020-11-24 | 江苏龙灯化学有限公司 | Weeding composition containing microcapsules and preparation method and application thereof |
| CN111972422B (en) * | 2019-05-21 | 2022-10-25 | 江苏龙灯化学有限公司 | Weeding composition containing microcapsules and preparation method and application thereof |
| CN111109251A (en) * | 2019-12-18 | 2020-05-08 | 中化化工科学技术研究总院有限公司 | Wetting dispersant and pendimethalin suspending agent using same |
| CN114246182A (en) * | 2021-12-30 | 2022-03-29 | 江苏仁信作物保护技术有限公司 | Pendimethalin microcapsule suspending agent and production process thereof |
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